An iterative approach was developed to determine the optimal monomer addition policies in real emulsion copolymerization systems in which only limited kinetic information is available. The approach was applied to obtain widely different copolymer composition profiles for the emulsion copolymerization of butyl acrylate and styrene. The approach involves a series of semicontinuous emulsion copolymerizations carried out in an open-loop control mode. Each reaction was used to obtain an estimation of the kinetics of the process that was used to calculate the monomer addition profiles for the next experiment. The method is model-independent and converges rapidly.